Process for obtaining sulphur



R. S. PERRY, P. W. WEBSTER, AND V. K. BOYNTON.

PROCESS FOR OBTAINING SULPHUR.

A?PLICATION FILED JULY 9.1920.

1,408,467. I Patented Mar- 7 1922.

5 $HEETS-SHEET I.

R. S. PERRY, P. W. WEBSTER, AND V. K. BOYNTON. PROCESS FOR OBTAINING SULPHUR.

APPLICATION FILED JULY 9,1920- Patented Mar. 7, 1922.

5 SHEETS-SHEET 2.

R. S. PERRY P. W. WEBSTER, AND V. K. BOYNTON.

PROCESS FOR OBTAINING SULPHUR.

APPLICATION FILED JULY 9,1920.

1,408,467. Patented Mar- 7, 1922. 5 SHEETSSHEET s.

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R. S. PERRY, P. W. WEBSTER, AND K. BOYNTON. PROCESS ron OBTAINING SULPHUR.

APPLICATION FILED JULY 9,1920. 1 ,408,4=67, Patented Mar. 7,1922.

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' 6110mm I Z I R. S. PERRY, P. W. WEBSTER, AND V. K. BOYNTON.

PROCESS FOR OBTAINING SULPHUR.

APPLICATION FILED JULY 9,1920.

1,408,467. e ed Mar 7, 1922.

5 SHEETSSHEET 5.

5] nvemrozs UNITED STATES PATENT (OFFICE.

ROB ERT S. PERRY, OF CAVE, SPRING, GEORGIA, AND PAUL W. WEBSTER, OF PELHAM MANOR, AND VERN K. BOYNTON, OF NEW YORK, N. Y., ASSIG-NORS T0 PERRY &

WEBSTER, me, or 'Ew'YoEK, N. Y.

To all whom it may concern:

Be it known that we, ROBERT S. PERRY, PAUL W. WEBSTER, and VERN K. BOYNTON, citizens of the United States, residing, respectively, in Cave Spring, county of Floyd, and State of Georgia, Pelham Manor, county of Westchester, and State of New York, and New York city, county of New York, and State of New York, have invented certain new and useful Improvements in Processes for Obtaining Sulphur, of which the following is a full, clear, and exact specification.

Our invention relates to the separation of sulphur from sulphur-containing materials and refers particularly to a process for the separation of sulphur from sulphur-containing materials through the medium of a heated liquid.

One object of our invention is' a process for the removal of sulphur. from sulphurcontaining materials by means of a heated liquid.

Another object of our invention is a continuous process for the recovery of practically pure sulphur from finely ground sulphur-containing materials and the continu-. ous separation of the spent material from the recovered sulphur.

Another object of our invention is a process for' the removal and recovery. of sulphur from sulphur-containing materials in which practically all of the heat necessary for the.

following out of the process may be recovered for a continuing of the process.

Another objectof our invention is a process for the removal of spent material from the sulphur extracted therefrom by passing the spent material through the molten sulphur.

The above and other objects of 011F111- vention will be evident upon a consideration of our specification and drawings.

Sulphur occurs in nature chiefly in the form of large deposits, usually at considerable depths below the surface, or in a 00- mingled condition with rocks and ores, which may be surface deposits or may be situated below the surface.

While the recovery of sulphur from ores comprisin complished with comparative ease, its re covery from ores in which it is co-mingled Specification of Letters Patent.

large deep deposits can be ac- PROCESS FOR OBTAINING SULPHUR. I

Patented Mar. '7, 1922.

Application filed July 9, 1920. Serial No. 895,105.

posed methods possess great difiiculties of operation as they result either in only partial extraction of the sulphuror the necessity of its further purification, in order to obtain it in the state of purity demanded by the trade.

Further, many of the proposed methods require large quantities of steam and as the sulphur-ore deposits are frequently situated great distances from the sources of suitable fuel supplies, such processes are commercially inoperative on account of the expense necessary for shipment of ore to place of fuel supply or for shipment of fuel to ore deposits. The'same difliculties present themselves in those methods in which large quantities of water are necessary for the production of steam, power, or for treating or washing purposes.

The process of our invention overcomes all of these difliculties and presents a method terials and possesses new and valuable features not found in previously proposed methods.

In a broad way, the process of our invention comprises a method whereby sulphur may be extracted from sulphur-containing materials by means of heated water and the spent materials and water removed from the sulphur by a movement of the water, the sulphur being in a practically pure condition.

By sulphur-containing materials we mean those materials which contain or carry sulphur, or have it" incorporated within them, in such a mechanicalor chemical condition that it can be extracted therefrom and the spent material removed from the sulphur by the process of our invention.

While the scope of our invention is not limited to any particular form of 'device, the details of construction of which maybe widely varied to, suit particular requirements, the accompanying drawings show one form of a device suitable for the carrying out of the process of our invention in which similar parts are designated by similar numerals.

Figure 1 is a diagrammatic elevation of one form of apparatus suitable for-the carrying out of the process of our invention.

igure 2 is a top plan view of Figure 1.

Figure 3 is a vertical section of the heater.

Figure 4 is a vertical section of the separator.

Figure 5 is a broken-vertical section'of the steam separator.

The device, as shown in the drawings, comprises a water-receptacle 10, connected by means of the pipe 11, carrying the valve 12, to the ore h0pper'13. The'hopper 13 opensinto the upper portion of the jacketed Y mixer 14, having the cover 15. The bottom portion of the mixer 14 is connected by means of the pipe 16 to the receiving end of the pump 17, the discharge end of which is connected by the pipe 18 to the upper portion' of thejacketed heater 19, having the cover 20. The bottom portion of the heater 19 is connected by means of the pipe 21 to the jacketed agglomeraton 22, having the cover 23. The bottom portion of the agglomerator 22 is connected by means of the pipe 24 to the lower portion of the jacketed separator 25 having the cover 26.' The bottom portion of the separator 25 carries the pipe 27, having the valve 28, opening into the raised end ofthe trough 29, the lower end of which opens into the lower end ofthe standard Dorr classifier 30 having the usually employed movable rakes 31, 31 connect'ed to the rake frame 32. 'A pipe-33 connects the classifier 30 tank 34.

the upper portion of the separator 25,with a steam separator comprising the enlarged pipe 37, connected with the, pipe 38, havlng' the wearing plate 39, thejlower end of thepipe 38' being situated within. the basin .40 and spaced from the bottom thereof. The

extended portion 41 of the basin 40 extends above and to the cefitral portion'of the thickwith the top of the j the separator.

ener, or settin tank,42. The bottom portion otthe t ickener 42 is connected by means of the pipe 43, carrying the valve 44,

to the upper portion of the tank 45, the lower portion of which carries the pipe 46, having the valve 47, leading to a dump or suitable place of deposit. A pipe 48, connected with asource ofwater supply, is coiled (49) within the tank 45 and is then extended into the pipe 50 opening into the top of the water tank 10. The upper portion of the thickener 42 is connected by means of the overflow pipe 51 to the to of the tank 34. 'A pipe 52, connected wit a source of water supply, enters the raised portion of the trough 29.

The upper portionof the pipe 38 is conpump 55, the discharge endof which iscon-. nected by means of the lpipe 56 with the top of the water tank 10. pipe 57, connected with a source of water supply, opens into the top of the 'water tank 10. i

A detailed drawing of the heater 19 is shown in Figure 3. This heater has jacketed walls, a suitable heating medium being capable of being introduced through the pipe 58 and withdrawn through the pipe 59. A suitable blade agitator 60 is fixedly attached to the revoluble shaft 61 passing through the stufiing box 62 within the cover 20, the upper end of the shaft 61, carrying the bevel gear 63, meshing with the bevel gear 64, carried by the revoluble shaft 65, the latter being connected to a source of revoluble power.

The agglomerator '22 is similar in con- .struction to the heater 19 and the mixer 14' is similar to the heater 19, except that the pipe 18 is replaced by the opening of the 4 67. The pipe 24 is connected with the pipe 68, which is extended downwardly and enters the hollow diaphragm member 69, which has a foraminous top 70, a clean-out plug 71 and is supported by the brackets 72, 72 fixedlg attached .to the walls of the separator.

ituated within the upper portion of the 3, 73, is an annular basin 74, having a central' openin .75 formed by the wall 76.01

U separator," andsup'ported by the brackets A pipe 35, carrying the valve 36, connects 7 the basin w ich is extended above the out side wall 77 of the basin.

The basin 74 is spaced from the walls of The pipe 35 extends down wardly through the cover 26, the end of the pipe 35 being spaced-from the bottom of the basin 74. An arm agitator 78 is fixedly 110 Lacketedwalls, a suitable heating medium 7 attached to the revoluble shaft 79, which passes through the stuffing box 80 in the cover 26. The upper end of the shaft 79 carries the fixedly attached bevel gear 81, meshing with the bevel gear 82, carried by the revoluble shaft 83 which, in turn, is connected with a source ofrevoluble power. The wall of the separator carries the clear vision glass 8 In the above description, we have applied the terms mixer, heater, agglomerator and separator to various parts of the drawings, simply as a ready means for designation and we do not mean to be understood that the mechanical operations indicated thereby are limited to the particular device I so designated.

\Ve give the following as an example of the carrying out of our process with the application thereof of the described devices A sulphur-containing materialcis reduced to about 80 mesh, or to such a degree of fineness as is sufficient to unlock and separate the sulphur in the subsequent operations,

and continuously introduced into the hopper 13 simultaneously with a stream of water through the pipe 11 from the tank 10, the proportions of the mixture being about five (5) parts of water to one (1) part of ore. The material and water pass into the mixer 14, in which they are thoroughly mixed by means of the agitator and are heated to a temperature below the boiling point of water by heating medium in the jacketed walls of the mixer. The heated mixture of material and water pass to the pump 17 whence they are forced through the pipe 18 into the heater 19, in which they are thoroughly mixed and heated to about 120 C. From the heater 19 the mixture passes through the pipe 21 into the agglomerator 22 in which the mixture is stirred and the temperature maintained at about 120 C. In the heater 19 and the agglomerator 22, the temperature of the mass causes the sulphur to melt and flow from the interstices of the ore, thus producing a mixture of spent material, or gangue, molten sulphur and water. While the general efiect produced in the heater and agglomerator are the same, that is, the melting of the sulphur and its separation from the ore, there is a specific effect produced in that the small globules of melted sulphur, first obtained in its extraction from the material, have a tendency to agglomerate into larger globules by the treatment and this agglomeration, which commences in the heater, is brought to a greater extent of completeness in the agglomerator. From the agglomerator 22 the mixture of spent material, sulphur more or less agglomerated and the water pas-s through the pipe 24 into the separator 25. The mixture passes through the pipes 24 and 68 into the dia- I in a molten condition.

phragm member 69 and thence outwardly through the foraminous top 70 into the separator, in which it is maintained at a temperature suflicient to retain the sulphur The heavier sulphur remains in the lower portionof the separator whereas the lighter gangue and water pass to the upper portion of the separator over the side 77 of, and into, the basin 74c and thence upwardly and outwardly through thepipe 35. The valve 28 of the pipe 27 is so set as to maintain a quantity of sulphur within the separator to a height represented approximately by the line AA'. It will thus be noted that all of the materials passing through the diaphragm 69 will pass upwardly through a molten mass of sulphur which will have a tendency to agglomerate and collect the molten sulphur thus introduced. The molten sulphur is; converted into its solid condition by passing through the pipe 27 into the trough "29, through which a constant flow of water is maintained by means of the pipe 52. The sulphur is thus obtained in a granulated condition particularly suitable for handling, storage and shipping. The water and sulphur pass from the trough 29 into the classifier 30, the sulphur thence passing upwardly and outwardly into suitable containers. The water introduced into the trough 29, and which has absorbed the heat of the molten sulphur, is carried to the tank 34 by means of the pipe 33. I

By means of the pump 17 and the proper regulation of the Valves 28 and 36, a predeflash into steam which passes through the pipe 50 to the' tank 10 for the purpose of heating the Water contained therein.

The gangue and hot water will pass downwardly through the pipe 38 into the basin f 40, and thence through the extended portion, or trough, 41, into the thickener 42.

The basin 40 is of sufficient height to produce by hydrostatic pressure of its contents a sufiicient pressure to force the steam through the pipe 53.

The gangue settles in the thickener 42 and thence passes outwardly through the pipe 43 into the tank 45 and thence outwardly through the pipe 46 to a desirable dump. By a regulationof the valves 44 and 4.7, the mass gangue may be maintained at a suitable height in the tank 45. Fresh wa ter passes through the pipe 48 and the coil 49, thus absorbing the heat of the gangue, and thence through the pipe 50 to'the tank 10. The hot overflow water from the thickener 42 passes through the pipe 51 to the tank 34 and the hot water in the tank 34:

passes through the pipe 54 to the pump 55 and thence is forced through the pipe 56 to the tank 10. The pipe 57 may be employed to introduce additional water into the tank 10, when the recovered Water is not suflicient for the continuance ofthe operation.

All of the devices, containers, pipes and parts may be covered with heat non-conducand that practically all of the heat necessary sulphur-containing material which com-'.

gangue and water in the following out of the method is recovered and returned thereto, thus reducing the amount of necessary heating material to a minnnum.

, It is further evident that while the process is described as continuous in-its operation, it may be employed in an intermittent manner and that the various steps of the operation may be used irrespective of a continuous process. i

We do not limit ourselves to theparticular chemicals, quantities, temperatures and se-.

quence of operative ste smentioned, nor to the particular devices escribed and shown, all of which may be varied without going beyond the scope of our inventionas described and claimed.

What we claim is-:

1. In a process of separating sulphur from a mixture of gangue, sulphur and water, the step which comprises passing the mixture'under pressure into a bath of molten sulphur, whereby the gangue and-water will pass therethrough accumulating sulphur of the mixture in the molten 2. The process of separating sulphur-from prises heating ainixture. of sulphur-containing material and water underpressure to a temperature sufiicient to melt the sulphur,

agitating the mixture until sulphur is separated from the material, passing the mixture into a b'ath'of molten sulphur, whereby the gangue and water will pass therethrough accumulating sulphur of the mix from contact withthe molten sulphun, a

3. The process of separating sulphur from sulphur-containing material -whichc'oi'n prises heatinga mixture ofsulphur-contaming material and water under pressure to a temperature suiiiclent' to melt the sulphur,

agitating the mixture until sulphur is up mass.

rated from the material, passing the mixture under pressure into a bath of moltenv sulphur, whereby the gangue and Water will pass therethrough accumulating sulphur of the mixture in the molten mass and removing the gangue and water from contact with the molten'sulphun- 4. The process of separating sulphur from sulphur containing material which comprises heating a mixture of sulphur-containing material and water under pressure to a temperature sufiicient to melt the sulphur, agitating the mixture until sulphur is separated from the material, passing the mixture under pressure into a bath of molten sulphur, whereby the gangue and water will pass-therethrough accumulating sulphur of the-,mixtureinthe molten mass, removing the gangue'and water from contact with the molten sulphur and returning practically all of-the employed caloric efiiciency to the first operation.

6; In a continuous process for the separation of sulphur from sulphur-bearing material the steps comprising a continuous progressivemovement ofa. mixture of sulphurbearing material and water, heating the mixture under pressure to the melting temperature of sulphur during said movement and causing a'movement of themixture during its progressive movement whereby sulphur will-be agglomerated intomolten masses withinthe mixture,

7. Ina continuous process for the separationof sulphur from sulphnr-bearlng materials the steps comprising lmmersing the finely ground -material in. water, causing a continuous progressive movement of the IDIX- ture, 1 182117111}; the, m xture under pressure during its progressiyemovement. until prac- 't ica 1ly allof' thejsiilphiir isextracted from ture in the moltenmass and removing'thea theme-termi s causing ai rnovement of the erated. into? molten masses within thei'mix f -'ture.. 1

. V 7 8: A continuous process for. the separation of sulphur from sulphurbearinglmaterial .which comprises a continuous pro ressive movement of ammo of sulphurive movement gun material and water, heating the mixture under pressure to the melting temperature of st lphur during said movement, causing a movement of the mixture during progressive movement whereby sulphur Wlll be ag-.

' glomerated into molten masses within the mlxture and separating the gangue and water from contact with the sulphur.

9. A continuous process for'the separation the mixture during its progressive moye- I so ment whereby extracted sulphur will be ag glomerated into molten masses within the mixture and separating the gangue and wafrom sulphur-containing material which ter from contact withthe sulphur. 10. A continuous process for the separation of sulphur 'from sulphur-bearing material which comprises a continuousprogres' sive movement of a mixture of sulphurbearing material and water, heating the mixture under pressure to the melting temperature of sulphur during said movement,

causing a movement of the mixture during its progressive movement whereby sulphur will be agglomerated into molten -masses gangue and water from the sulphur by passing the mixture into a bath of molten sulphur whereby the gangue and water will pass therethrough accumulating sulphur in the molten mass.

11. A continuous process for the separation of sulphur from sulphur-bearing materials which comprises immersing the finely ground material in water, causing a continuous progressive movement of the mixture, heating the mixture under pressure during its progressive movement until practicallyall of the sulphur is extracted from the material, causing a movement'of the mixture during its progressive movement,

whereby extracted sulphur will be agglomeratedinto molten masses within the mixture-and separating the gangue andw water from the sulphur by passing the mixture intoa bath of molten sulphur whereby the gangue and water will pass therethrough ac cumulating sulphur in the molten'mass.

12.;Acontinuous process for the separation of'sulphur from a sulphur-containing material which comprises, heating under pressure a mixture of a sulphur-containing -material and water to a temperature of about 120 C. causing a movement of the mixture whereby the extracted sulphur will agglomerate into a molten mass and removing the material and water from contact with the sulphur. J I

-13."The process of separating sulphur comprises heating a mixture of sulphur-containing material and water under pressure {to a temperature sufli'cient to melt the sulphur and passing the heated mixture under presj taining material and water under pressure to within the mixture and separating the and separating the spent material and water from the sulphur.

Signed at New York in the county of New York and State of New York, this 1st day of July, 1920.

ROBERT s. PERRY. PAUL W. WEBSTER. VERN K. BOYNTON. 

